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Monodisperse titanium dioxide nanometer microballoons and preparation method thereof

A technology of titanium dioxide and nano-microspheres is applied in the fields of nanomaterials and photocatalysis, which can solve the problems of large specific surface area, and achieve the effects of uniform size distribution of microspheres, good crystallization, and reduced difficulty.

Inactive Publication Date: 2012-05-02
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, by using the reaction between metal titanium and hydrogen peroxide solution, titanium dioxide films in various forms such as nanoporous, nanowire, nanorod, nanoflower, etc. have been prepared, but there is no reaction between metal titanium and hydrogen peroxide solution to obtain a large specific surface area. monodisperse titanium dioxide nanospheres

Method used

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  • Monodisperse titanium dioxide nanometer microballoons and preparation method thereof
  • Monodisperse titanium dioxide nanometer microballoons and preparation method thereof
  • Monodisperse titanium dioxide nanometer microballoons and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0027] 1) Mix hydrofluoric acid, 65% nitric acid and deionized water with a mass concentration of 55% in a volume ratio of 1:3:6 to obtain a pickling solution;

[0028] 2) The size is 5×5×0.01(cm 3 ) The surface of the metal titanium plate is pickled with the pickling solution obtained in step 1), then cleaned in ultrasonic waves with deionized water, immersed in 50ml of hydrogen peroxide with a mass concentration of 30%, and taken out after reacting at 80°C for 12 hours A metal titanium plate is obtained to obtain a precursor solution containing tetravalent titanium ions;

[0029] 3) Sodium hydroxide was added to the precursor solution to form a sodium hydroxide solution with a concentration of 5 mol / liter, which was placed in a polytetrafluoroethylene hydrothermal tank, and hydrothermally reacted at 120° C. for 20 hours to obtain a powder. The volume ratio of reaction liquid and hydrothermal tank is 4: 5;

[0030] 4) The powder was washed three times repeatedly with deioni...

Embodiment 2

[0033] 1) with embodiment 1;

[0034] 2) with embodiment 1;

[0035] 3) Add sodium hydroxide to the precursor solution to form a sodium hydroxide solution with a concentration of 10 mol / liter, put it into a polytetrafluoroethylene hydrothermal tank, and conduct a hydrothermal reaction at 120° C. for 40 hours to obtain a powder.

[0036] 4) The powder was repeatedly washed with deionized water for 3 times, then soaked in 0.6 mol / L dilute hydrochloric acid solution for 12 hours, dried, and put into a muffle furnace for heat treatment at 600° C. for 1 hour to obtain monodisperse titanium dioxide nanospheres.

[0037] Depend on image 3 It can be seen that the obtained monodisperse titanium dioxide nano-microspheres have a diameter of 1.5-2.5 micrometers and are composed of nanowire clusters with a length of 600 nanometers and a diameter of 30 nanometers.

[0038] Figure 4 The high-resolution transmission electron microscopy images of monodisperse titanium dioxide nanospheres ...

Embodiment 3

[0040] 1) with embodiment 1;

[0041] 2) The size is 5×5×0.01(cm 3 ) The surface of the metal titanium plate is pickled with the pickling solution obtained in step 1), then cleaned in ultrasonic waves with deionized water, immersed in 50ml of hydrogen peroxide with a mass concentration of 30%, and reacted at 80°C for 24 hours to take out the metal Titanium plate to obtain a precursor solution containing tetravalent titanium ions;

[0042] 3) Add sodium hydroxide to the precursor solution to form a sodium hydroxide solution with a concentration of 5 mol / liter, put it into a polytetrafluoroethylene hydrothermal tank, and conduct a hydrothermal reaction at 120° C. for 64 hours to obtain a powder.

[0043] 4) with embodiment 2.

[0044] Depend on Figure 6 It can be seen that the obtained monodisperse titanium dioxide nano-microspheres have a diameter of 1.5-2.5 microns and are composed of nanowire clusters with a length of 800 nanometers and a diameter of 40 nanometers.

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Abstract

The invention discloses monodisperse titanium dioxide nanometer microballoons and a preparation method thereof. The diameters of the nanometer microballoons are 1.5-2.5 micrometers, and the microballoons have uniform size, good dispersity and high specific surface area. The single microballoon is formed by clustering nanometer wires with a length of 0.5-1.0 micrometer and a diameter of 20-50 nanometers. A reaction system consists of a residual solution left after a metal titanium plate reacts with hydrogen peroxide and a sodium hydroxide solution and is subjected to a hydro-thermal reaction for 20-64 hours at 120 DEG C to prepare the microballons; and after adopting subsequent proton exchange and heat treatment at 450-700 DEG C, the nanometer microballoons are crystallized into anatase. In the presence of the same condition, the efficiency of the nanometer microballoons subjected to heat treatment at 600 DEG C for assisting photocatalysis to degrade rhodamine B dye in water is obviously superior to that of commercial titanium dioxide nanometer powder Degussa P25.

Description

technical field [0001] The invention relates to titanium dioxide nano microspheres and a preparation method thereof, and belongs to the technical field of nanometer materials and photocatalysis. Background technique [0002] As one of the advanced oxidation technologies, titanium dioxide photocatalytic technology utilizes the strong oxidizing properties of photogenerated holes induced by photons to non-selectively deep-oxidize various organic pollutants in sewage, so it is an ideal sewage treatment technology. The crystal form, specific surface area and morphology of titanium dioxide are the key factors to determine its photocatalytic efficiency. Titanium dioxide with anatase structure has more excellent photocatalytic performance than other crystal forms such as rutile and brookite. At the same time, the different morphology of titanium dioxide affects its specific surface area, which also has an important impact on the adsorption of organic pollutants and the separation a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G23/053
Inventor 吴进明宋小梅
Owner ZHEJIANG UNIV
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